CN114275735B - Mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder material and preparation method thereof - Google Patents
Mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder material and preparation method thereof Download PDFInfo
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- CN114275735B CN114275735B CN202111626296.4A CN202111626296A CN114275735B CN 114275735 B CN114275735 B CN 114275735B CN 202111626296 A CN202111626296 A CN 202111626296A CN 114275735 B CN114275735 B CN 114275735B
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Abstract
The invention belongs to the technical field of hydrogen storage materials, and particularly relates to Mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder and a preparation method thereof x (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 1‑x Wherein x =0.01 to 0.25. The invention successfully prepares Mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder and Mg prepared by the method x (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 1‑x The content of Mg which can be added into the high-entropy alloy powder can reach 25 percent at most, and compared with the traditional high-entropy alloy, a large amount of light element Mg is added, so that the density of the alloy is greatly reduced; mg prepared simultaneously x (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 1‑x The high-entropy alloy powder has the characteristics of reversible hydrogen storage at room temperature and high cycle stability, and has the outstanding effect of reversible hydrogen absorption and desorption at room temperature compared with other Mg-containing high-entropy alloys; the preparation method is simple and easy to control, the investment of production equipment is low, the production process is pollution-free, and the industrial large-scale production is easy to realize.
Description
Technical Field
The invention belongs to the technical field of hydrogen storage materials, and particularly relates to a Mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder material and a preparation method thereof.
Background
The hydrogen storage alloy can absorb and release hydrogen under certain conditions, and is a safe and efficient hydrogen storage material. Hydrogen storage alloys can be classified into the following categories: rare earth system AB 5 Type alloy (LaNi) 5 ) (ii) a Mg-based hydrogen storage alloy (Mg and Mg) 2 Ni); titanium AB type alloys (Ti-Fe, ti-Mn); laves phase AB 2 Type alloy (ZrMn) 2 、MgZn 2 )；AB 3 Hydrogen storage alloy (PrNi) 3 La-Mg-Ni) and V group have a BCC (body centered cubic) structure. The high-entropy alloy consists of a plurality of alloy elements and has the properties of the alloy elementsAn alloy of (2). Theoretically, it is possible to obtain hydrogen storage properties in a high entropy alloy by adding an alloy element capable of storing hydrogen to the high entropy alloy and forming a BCC solid solution structure.
In terms of hydrogen storage performance, the hydrogen storage capacity of the conventional hydrogen storage high-entropy alloy is generally lower than 2.0wt%, mainly because a large amount of heavy metal elements (such as Zr, nb, mo, hf and Ta) are added in the design for hydrogen storage, which is not favorable for obtaining high hydrogen storage capacity. The existing hydrogen storage high-entropy alloy design is mainly improved on the basis of the tradition, and the hydrogen storage capacity is improved by replacing heavy metal elements with transition metal elements. Compared with transition metal elements, mg has the advantages of high hydrogen storage capacity (7.6 wt% of theoretical hydrogen storage capacity), low density, wide sources and low price, and the addition of Mg into the high-entropy alloy and the formation of BCC solid solution can better reduce the density of the high-entropy alloy and has the possibility of further improving the hydrogen storage capacity.
However, high entropy alloys containing Mg present many difficulties in their preparation: firstly, the steam pressure of Mg is high, and the preparation of the Mg-containing high-entropy alloy by the traditional arc melting and induction melting method can cause a large amount of burning loss of Mg, so that the accurate control of the components of the high-entropy alloy and the industrial production are not facilitated; secondly, the crystal structure of Mg is an HCP (hexagonal close packing) structure, and the atomic radius of Mg is larger than that of transition group metals, and therefore, it is difficult to form a BCC solid solution containing Mg.
Mechanical alloying is one of conventional methods for preparing high-entropy alloy, the existing research mainly adopts a common planetary ball milling method to prepare magnesium-containing high-entropy alloy, and MgAlTiFeNi and other alloys are recently developed in the aspect of Mg-containing high-entropy alloy. These high entropy alloys are deficient in the following respects: 1) Most of the prepared high-entropy alloy contains impurity phases (such as various alloy phases and compound phases); 2) The high-entropy alloy is easy to generate hydrogen-induced decomposition during hydrogen absorption and desorption, and has poor hydrogen absorption and desorption reversibility; 3) The hydrogen releasing temperature of the alloy is too high, and the alloy can be rapidly released at the temperature of more than 300 ℃.
Therefore, how to design the Mg-containing high-entropy alloy capable of reversibly absorbing and releasing hydrogen at room temperature has important practical application value.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a Mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder material and a preparation method thereof. The Mg-containing high-entropy hydrogen storage alloy powder has the hydrogen storage capacity of 0.42 to 0.46 weight percent at room temperature; the biphase Mg-containing room temperature reversible hydrogen storage high-entropy alloy has the characteristics of simple preparation process, high efficiency, high yield, no pollution and the like, the maximum Mg content of the alloy can reach 25%, and the biphase Mg-containing room temperature reversible hydrogen storage high-entropy alloy has the remarkable advantage of rapid room temperature reversible hydrogen storage.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder material with the chemical formula of Mg x (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 1-x Wherein x =0.01 to 0.25.
The preparation method of the Mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder material comprises the following steps:
1) Weighing five raw material metal powders of Mg, ti, V, nb and Cr according to a ratio, pouring the weighed raw material metal powders into a ball milling tank in a glove box, adding grinding balls according to a certain ball-material ratio, and then pouring n-heptane to submerge the grinding balls;
2) Sealing the ball milling tank, putting the ball milling tank on a high-speed vibration ball mill, carrying out wet milling for a period of time, and cooling to room temperature after the wet milling is finished;
3) And taking down the ball milling tank cover in the glove box, and removing n-heptane to obtain the Mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder material.
Further, in the step 1), the purity of Mg powder is more than or equal to 99.5 percent, the purity of Ti, V, nb and Cr raw material metal powder is more than or equal to 99 percent, and the granularity of all the raw material powder is not less than 200 meshes.
Further, in the step 1), the ball-to-feed ratio is 20-30.
Further, in the step 1), the purity of the n-heptane is more than or equal to 99%.
Further, in the step 2), the ball milling tank is a stainless steel ball milling tank, the grinding balls are stainless steel grinding balls, and the feeding operation is carried out in a glove box.
Further, in the step 2), the wet grinding time is 30-40 h.
Further, in the step 2), the shimmying frequency of the n-heptane high-speed vibration ball mill is 1200 weeks/min, and the shimmying stops for 10min every 30min of operation.
Further, in the step 3), the operation of removing n-heptane is as follows: and (4) pumping out n-heptane above the powder by using a rubber head dropper, and removing the residual small amount of n-heptane by adopting a transition bin vacuumizing method.
Furthermore, the time for vacuumizing the transition bin is 1-2 h.
The alloy design aspect of the invention is improved on the basis of the equal atomic ratio TiVNbCr, on the basis of ensuring the general design principle of high-entropy alloy design (delta is less than 10 percent, -15 is less than delta Hmix is less than 5kJ/mol, and omega is more than or equal to 1.1), the content of Cr element with small atomic radius is reduced to 10 percent, the average atomic radius of the alloy is improved, and Mg is convenient to add; slightly reducing the content of Nb element with higher density; by the adjusting mode, the light element Mg with larger atomic radius can be added into the alloy more easily, and the density of the alloy is reduced; the addition of the alloying element Mg can significantly reduce the density of the alloy. The preparation method adopts a high-speed vibration ball method, the high-speed vibration ball milling is a novel mechanical alloying method combining planetary motion and vertical high-frequency vibration, the materials are impacted, rubbed and sheared through the composite complex high-energy motion, the mutual diffusion and the interaction among atoms are greatly promoted, the mixing entropy of a material system is greatly increased, and the formation of the multi-component high-entropy alloy is facilitated.
The invention has the beneficial effects that:
1. the invention successfully prepares Mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder and Mg prepared by the method x (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 1-x The content of Mg which can be added into the high-entropy alloy powder can reach 25 percent at most, and compared with the traditional high-entropy alloy, a large amount of light element Mg is added, so that the density of the alloy is greatly reduced.
2. Mg prepared by the invention x (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 1-x The high-entropy alloy powder has the characteristics of reversible hydrogen storage at room temperature and high cycle stability, and compared with other Mg-containing high-entropy alloys, the high-entropy alloy powder has the outstanding effect of reversible hydrogen absorption and desorption at room temperature.
3. The preparation method is simple and easy to control, the investment of production equipment is low, the production process is pollution-free, and the industrial large-scale production is easy to realize.
Of course, it is not necessary for any one product that embodies the invention to achieve all of the above advantages simultaneously.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is Mg 0.1 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.9 X-ray diffraction pattern of Mg-containing high-entropy alloy powder;
FIG. 2 is Mg 0.1 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.9 A hydrogen absorption and desorption diagram of Mg-containing high-entropy alloy powder;
FIG. 3 is Mg 0.2 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.8 X-ray diffraction pattern of Mg-containing high-entropy alloy powder;
FIG. 4 is Mg 0.2 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.8 A hydrogen absorption and desorption diagram of Mg-containing high-entropy alloy powder;
FIG. 5 is Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 X-ray diffraction pattern of the high-entropy alloy powder;
FIG. 6 is Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 High-entropy alloy powderA hydrogen absorption and desorption diagram;
FIG. 7 is a graph of hydrogen absorption capacity for 10 cycles of the high-entropy alloy powder.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The specific embodiment of the invention is as follows:
example 1
Press Mg in glove box 0.1 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.9 Respectively weighing 5 g of Mg (granularity 200 meshes, purity 99.5 percent), ti, V, nb and Cr powder (granularity 200 meshes, purity 99 percent). Putting the weighed elemental metal powder into a stainless steel ball-milling tank, adding stainless steel grinding balls according to the ball-material ratio of 20. And (3) placing the ball milling tank in a high-speed vibration ball mill for wet ball milling for 30 hours, wherein the pendulum vibration frequency of the ball mill is 1200 weeks/minute, and the ball mill stops for 10 minutes every 30 minutes. After the ball milling is finished, pumping out n-heptane above the powder by using a rubber head dropper in a glove box, removing the residual n-heptane by adopting a transition bin vacuumizing method for 1h to obtain Mg consisting of FCC/BCC biphase 0.1 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.9 Two-phase Mg-containing high-entropy hydrogen storage alloy powder (see fig. 1 0.1 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.9 X-ray diffraction pattern of two-phase Mg-containing high-entropy alloy powder). The high entropy alloy powder was able to reversibly store hydrogen at room temperature with a capacity of about 0.44wt.% (see fig. 2 mg 0.1 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.9 Hydrogen absorption and desorption diagram of Mg-containing high-entropy alloy powder); hydrogen uptake was cycled 10 times at room temperature with a reversible capacity of 94% (see FIG. 7)b：Mg 0.1 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.9 High entropy alloy powder 10 times cycle hydrogen absorption capacity graph).
Example 2
In glove box press Mg 0.2 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.8 Respectively weighing 5 g of Mg (granularity 200 meshes, purity 99.5 percent), ti, V, nb and Cr powder (granularity 200 meshes, purity 99 percent). Putting the weighed elemental metal powder into a stainless steel ball milling tank, adding stainless steel grinding balls according to the ball-material ratio of 20. And (3) placing the ball milling tank in a high-speed vibration ball mill for wet ball milling for 30 hours, wherein the pendulum vibration frequency of the ball mill is 1200 weeks/minute, and the ball mill stops for 10 minutes every 30 minutes. After the ball milling is finished, pumping out n-heptane above the powder by using a rubber head dropper in a glove box, removing the residual n-heptane by adopting a transition bin vacuumizing method for 2 hours to obtain Mg consisting of FCC/BCC biphase 0.2 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.8 Two-phase Mg-containing high-entropy hydrogen storage alloy powder (see fig. 3 Mg 0.2 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.8 High entropy alloy powder X-ray diffraction pattern). The high entropy alloy powder is capable of reversible hydrogen storage at room temperature with a capacity of about 0.42wt.% (see fig. 4): mg (Mg) 0.2 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.8 A hydrogen absorption and desorption diagram of Mg-containing high-entropy alloy powder; hydrogen was absorbed 10 times cyclically at room temperature with a reversible capacity of 94.7% (see FIG. 7 c: mg) 0.2 (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) 0.8 High entropy alloy powder 10 times cycle hydrogen absorption capacity plot).
Comparative example
Press Ti in glove box 0.35 V 0.35 Nb 0.2 Cr 0.1 The components (A) are 5 g of Ti, V, nb and Cr powders (granularity 200 mesh, purity 99%) are weighed respectively. Putting the weighed simple substance metal powder into a stainless steel ball milling tank, adding stainless steel grinding balls according to the ball material ratio of 20The alkane (purity greater than 99%) is immersed in the stainless steel ball, and the ball mill cover is sealed. And (3) placing the ball milling tank in a high-speed vibration ball mill for wet ball milling for 40 hours, wherein the pendulum vibration frequency of the ball mill is 1200 weeks/minute, and the ball mill stops for 10 minutes every 30 minutes. After the ball milling is finished, pumping out n-heptane above the powder by using a rubber head dropper in a glove box, removing the residual n-heptane by adopting a transition bin vacuumizing method for 2 hours to obtain Ti consisting of FCC/BCC biphase 0.35 V 0.35 Nb 0.2 Cr 0.1 Two-phase high-entropy hydrogen storage alloy powder. (see FIG. 5 0.35 V 0.35 Nb 0.2 Cr 0.1 High entropy alloy powder X-ray diffraction pattern); the high entropy alloy powder is capable of reversible hydrogen storage at room temperature with a capacity of about 0.46wt.% (see 6 ti 0.35 V 0.35 Nb 0.2 Cr 0.1 Hydrogen absorption and desorption diagram of Mg-containing high-entropy alloy powder); hydrogen was absorbed 10 times cyclically at room temperature with a reversible capacity of 93% (see FIG. 7 a: ti) 0.35 V 0.35 Nb 0.2 Cr 0.1 High entropy alloy powder 10 times cycle hydrogen absorption capacity plot).
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand the invention for and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (9)
1. A Mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder material is characterized in that: the chemical formula of the material is Mg x (Ti 0.35 V 0.35 Nb 0.2 Cr 0.1 ) x1- Wherein x =0.01 to 0.25.
2. The preparation method of the Mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder material according to claim 1, characterized by comprising the following steps:
1) Weighing five raw material metal powders of Mg, ti, V, nb and Cr according to a ratio, pouring the weighed raw material metal powders into a ball milling tank in a glove box, adding grinding balls according to a certain ball-material ratio, and then pouring n-heptane to submerge the grinding balls;
2) Sealing the ball milling tank, putting the ball milling tank on a high-speed vibration ball mill, carrying out wet milling for a period of time, and cooling to room temperature after the wet milling is finished;
3) And taking down the cover of the ball milling tank in the glove box, and removing n-heptane to obtain the Mg-containing room-temperature reversible hydrogen storage high-entropy alloy powder material.
3. The method of claim 2, wherein: in the step 1), the purity of Mg powder is more than or equal to 99.5 percent, the purity of Ti, V, nb and Cr raw material metal powder is more than or equal to 99 percent, and the granularity of all the raw material powder is not less than 200 meshes.
4. The production method according to claim 2, characterized in that: in the step 1), the ball-material ratio is 20-30.
5. The method of claim 2, wherein: in the step 1), the purity of the n-heptane is more than or equal to 99%.
6. The production method according to claim 2, characterized in that: in the step 2), the wet milling time is 30-40 h.
7. The method of claim 2, wherein: in the step 2), the shimmying frequency of the n-heptane high-speed vibration ball mill is 1200 weeks/min, and the shimmying is stopped for 10min every 30min of operation.
8. The method of claim 2, wherein: in the step 3), the operation of removing the n-heptane comprises the following steps: and (4) extracting n-heptane above the powder by using a rubber head dropper, and removing the residual n-heptane by adopting a transition bin vacuumizing method.
9. The method of claim 8, wherein: the vacuumizing time is 1-2 h.
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